Ethylene Glycol → HCID 20328332, compound

HRID 1973099Notes

Reaction equation

HRID 1973099 reaction equation
C([N:6]1[CH2:11][CH2:10][N:9]([CH:12]2[C:18]3[CH:19]=[C:20]([F:23])[CH:21]=[CH:22][C:17]=3[S:16][C:15]3[CH:24]=[CH:25][C:26]([CH3:28])=[CH:27][C:14]=3[CH2:13]2)[CH2:8][CH2:7]1)(OCC)=O.C(O)CO.[OH-].[K+]>O>[F:23][C:20]1[CH:21]=[CH:22][C:17]2[S:16][C:15]3[CH:24]=[CH:25][C:26]([CH3:28])=[CH:27][C:14]=3[CH2:13][CH:12]([N:9]3[CH2:10][CH2:11][NH:6][CH2:7][CH2:8]3)[C:18]=2[CH:19]=1

Participants

5

Reactant 3

HCID 174Ethylene GlycolHCID 14797Potassium HydroxideHCID 20328334HCID 20328334, compound

Product 1

HCID 20328332HCID 20328332, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent2×

Procedure

24.5 G. of 1-carbethoxy-4-[8-fluoro-10,11-dihydro-2-methyl-dibenzo[b,f]thiepin-10-yl]-piperazine, 350 ml. of ethyleneglycol, 19 g. of potassium hydroxide and 15 ml. of water are heated at 160° C. for 1 hour. The mixture is poured into water and extracted with chloroform. The organic phase is washed with water, dried over magnesium sulfate, evaporated under reduced pressure, and there is obtained 1-[8-fluoro-10,11-dihydro-2-methyl-dibenzo[b,f]thiepin-10-yl]-piperazine as a light-brown oil.

Workup

  1. extractionextracted with chloroform
  2. washThe organic phase is washed with water
  3. dry with materialdried over magnesium sulfate
  4. customevaporated under reduced pressure

Sources & evidence

ORD record
ord-98b71d831cf94aba8b6c6baaac55cb09
Source dataset
uspto-grants-1976_12
Patent number
US03996229

Reaction notes

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